TWI697565B - Method for recovering gold-containing titanium-aluminum sputtering derived resources - Google Patents

Method for recovering gold-containing titanium-aluminum sputtering derived resources Download PDF

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TWI697565B
TWI697565B TW108115293A TW108115293A TWI697565B TW I697565 B TWI697565 B TW I697565B TW 108115293 A TW108115293 A TW 108115293A TW 108115293 A TW108115293 A TW 108115293A TW I697565 B TWI697565 B TW I697565B
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titanium
aluminum
gold
recovery
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TW202041682A (en
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李清華
張家興
鍾鈺堂
林靖軒
李連耀
蘇瑞鴻
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滿益金科技有限公司
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Abstract

本發明涉及一種含金、鈦、鋁濺鍍衍生資源物回收方法,係提供回收金、鈦、鋁等金屬資源,其包含有:一回收鋁步驟,係將以一資源物放入20~30℃的氫氧化鈉浸漬劑中,並浸漬15~25分鐘後,過濾後而得一含鋁浸漬液及一含金、鈦濾渣,再將該含鋁浸漬液經過pH調整沉澱後,即得氫氧化鋁回收物;一回收金步驟,係將前述含金、鈦濾渣放入60~80℃的硝酸浸漬劑中,並浸漬3~5小時後,過濾而得高純度金回收物及一含鈦浸漬液;一回收鈦步驟,係將該含鈦浸漬液經過pH調整沉澱後,即得氫氧化鈦回收物。 The invention relates to a method for recovering resources derived from gold, titanium, and aluminum sputtering, which provides the recovery of metal resources such as gold, titanium, aluminum, etc., and includes: a step of recovering aluminum, in which a resource is placed in 20-30 After being immersed in sodium hydroxide impregnant at ℃ for 15-25 minutes, filtered to obtain an aluminum-containing impregnating solution and a gold and titanium-containing filter residue. After the aluminum-containing impregnating solution is adjusted and precipitated by pH, hydrogen is obtained. Alumina recovery; a gold recovery step involves putting the aforementioned gold and titanium filter residue into a nitric acid impregnant at 60-80°C, and immersing for 3 to 5 hours, and then filtering to obtain a high-purity gold recovery and a titanium-containing Impregnating solution; a step of recovering titanium, after the titanium-containing impregnating solution undergoes pH adjustment and precipitation, the recovered titanium hydroxide is obtained.

Description

含金鈦鋁濺鍍衍生資源物回收方法 Recovery method of resources derived from gold-containing titanium-aluminum sputtering

本發明涉及一種含金廢棄物回收技術,尤指回收含金、鈦、鋁濺鍍衍生資源物之技術範疇。 The invention relates to a gold-containing waste recycling technology, in particular to the technical category of recycling resources derived from gold, titanium, and aluminum sputtering.

現代面臨金屬資源短缺、黃金價格居高不下,如何從製程衍生物回收高純度黃金供產業使用,據以發展現代煉金術,不但能解決都市廢棄物對環境的汙染,更可創造資源再生的產值。 Modern times are facing a shortage of metal resources and the price of gold remains high. How to recover high-purity gold from process derivatives for industrial use and to develop modern alchemy can not only solve the environmental pollution of municipal waste, but also create resource regeneration output value .

按,一般物理氣相沉積(Physical vapor deposition,簡稱PVD),又稱真空濺鍍,係以濺鍍方式將各種金屬材質鍍膜在水五金、自行車零組件、3C產品、精品上,而獲得絕佳的外觀表面;換言之,濺鍍製程會產生「含金、鈦、鋁濺鍍衍生資源物」,具有回收價值。 According to, general physical vapor deposition (PVD), also known as vacuum sputtering, is to coat various metal materials on water hardware, bicycle components, 3C products, and boutique products by sputtering, and obtain excellent results. In other words, the sputtering process will produce "resources derived from gold, titanium, and aluminum sputtering", which has recycling value.

緣此,本發明人乃窮極心思開發出一種含金、鈦、鋁濺鍍衍生資源物回收方法,故本發明之目的:在於提供可同時回收金、鈦、鋁濺鍍衍生資源物之回收方法;故本發明之另一目的:在於提供回收流程簡化、安全性較高之含金、鈦、鋁濺鍍衍生資源物回收方法。 For this reason, the inventors worked hard to develop a recovery method for sputter-derived resources containing gold, titanium, and aluminum. Therefore, the purpose of the present invention is to provide a recovery method that can simultaneously recover gold, titanium, and aluminum sputter-derived resources. ; Therefore, another objective of the present invention is to provide a method for recycling sputtering-derived resources containing gold, titanium, and aluminum with a simplified recycling process and high safety.

本發明為達上述目的,運用了如下技術手段: 關於一種含金、鈦、鋁濺鍍衍生資源物回收方法,係包含有:一回收鋁步驟,係將以一資源物放入20~30℃的氫氧化鈉(NaOH)浸漬劑中,並浸 漬15~25分鐘後,過濾後而得一含鋁浸漬液及一含金、鈦濾渣,再將該含鋁浸漬液經過pH調整沉澱後,即得氫氧化鋁Al(OH)3回收物;一回收金步驟,係將前述含金、鈦濾渣放入60~80℃的硝酸(HNO3)浸漬劑中,並浸漬3~5小時後,過濾而得高純度金回收物及一含鈦浸漬液;一回收鈦步驟,係將該含鈦浸漬液經過pH調整沉澱後,即得氫氧化鈦Ti(OH)4回收物。 To achieve the above objective, the present invention uses the following technical means: Regarding a recovery method for sputtering derived resources containing gold, titanium, and aluminum, it includes: a step of recovering aluminum, which is to place a resource at 20-30°C After being immersed in sodium hydroxide (NaOH) impregnant for 15-25 minutes, filtered to obtain an aluminum-containing impregnating solution and a filter residue containing gold and titanium, and then the aluminum-containing impregnating solution is adjusted and precipitated by pH adjustment. Obtain aluminum hydroxide Al(OH) 3 recovery; a gold recovery step is to put the aforementioned gold and titanium filter residue into a nitric acid (HNO 3 ) impregnant at 60~80℃, and immerse for 3~5 hours, then filter A high-purity gold recovery product and a titanium-containing impregnation solution are obtained; a titanium recovery step is to obtain titanium hydroxide Ti(OH) 4 recovery product after the titanium-containing impregnation solution undergoes pH adjustment and precipitation.

所述含金、鈦、鋁濺鍍衍生資源物回收方法,其中在該回收鋁步驟之前,先經過一破碎處理步驟。 In the method for recovering resources derived from sputtering containing gold, titanium, and aluminum, a crushing treatment step is performed before the aluminum recovery step.

所述含金、鈦、鋁濺鍍衍生資源物回收方法,其中在該回收鋁步驟中所使用氫氧化鈉浸漬劑濃度設為5N~6N,且其浸漬固液比條件設為3g/100ml,但其浸漬劑濃度、浸漬固液比及浸漬時間等條件可以有多種搭配方式,並非為絕對。 In the recovery method of sputtering derived resources containing gold, titanium and aluminum, the concentration of the sodium hydroxide impregnant used in the aluminum recovery step is set to 5N-6N, and the impregnation solid-liquid ratio condition is set to 3g/100ml, However, the impregnant concentration, impregnation solid-liquid ratio, and impregnation time can be matched in many ways, which are not absolute.

所述含金、鈦、鋁濺鍍衍生資源物回收方法,其中在該回收鋁步驟中的pH調整沉澱方式,係以鹽酸(HCl)溶液調節該含鋁浸漬液的酸鹼值至pH7。 In the method for recovering resources derived from sputtering containing gold, titanium, and aluminum, the pH adjustment and precipitation method in the aluminum recovery step is to adjust the acid-base value of the aluminum-containing impregnation solution to pH 7 with a hydrochloric acid (HCl) solution.

所述含金、鈦、鋁濺鍍衍生資源物回收方法,其中在該回收金步驟中所使用硝酸(HNO3)浸漬劑濃度設為5N~6N,且其浸漬固液比條件設為1g/100ml,但其浸漬劑濃度、浸漬固液比及浸漬時間等條件可以有多種搭配方式,並非為絕對。 In the method for recovering gold, titanium, and aluminum sputtering-derived resources, the concentration of the nitric acid (HNO 3 ) impregnant used in the gold recovery step is set to 5N-6N, and the impregnation solid-to-liquid ratio condition is set to 1g/ 100ml, but the impregnant concentration, impregnation solid-liquid ratio and impregnation time can be matched in many ways, which is not absolute.

所述含金、鈦、鋁濺鍍衍生資源物回收方法,其中在該回收鈦步驟中的pH調整沉澱方式,係以氫氧化鈉(NaOH)溶液調節該含鈦浸漬液的酸鹼值至pH7。 The method for recovering resources derived from gold, titanium, and aluminum sputtering, wherein the pH adjustment precipitation method in the step of recovering titanium is to adjust the acid-base value of the titanium-containing impregnating solution to pH 7 with sodium hydroxide (NaOH) solution .

本發明運用上述技術手段,可以達到如下功效: The present invention uses the above technical means to achieve the following effects:

1.每片金、鈦、鋁濺鍍衍生資源物的有價金屬比例大約是金30%、鈦10%、鋁60%,使用本發明回收技術可以達到零廢棄的完全回收;目前金每公斤市價140萬元,鈦每公斤市價220元,鋁每公斤市價60元,一方面讓有價金屬可以再次被利用,增加經濟收益。 1. The proportion of valuable metals in each piece of gold, titanium, and aluminum sputtering derived resources is about 30% gold, 10% titanium, and 60% aluminum. The use of the recycling technology of the present invention can achieve complete recycling with zero waste; the current market price of gold per kilogram 1.4 million yuan, the market price of titanium is 220 yuan per kilogram, and the market price of aluminum is 60 yuan per kilogram. On the one hand, valuable metals can be used again and increase economic benefits.

2.本發明的回收方法簡化,各步驟流程的操作條件簡單,可降低其回收成本,而且免用腐蝕性強的王水,而以濕式冶鍊法回收取下鋁、鈦,不需要用高危險的化學物質來溶金,屬於友善環境的綠色技術。 2. The recovery method of the present invention is simplified, the operating conditions of each step of the process are simple, the recovery cost can be reduced, and the corrosive aqua regia is not used, and the aluminum and titanium are recovered and removed by the wet metallurgical chain method. Highly dangerous chemicals to dissolve gold are environmentally friendly green technologies.

A:含金、鈦、鋁濺鍍衍生資源物回收方法 A: Recovery method of sputtering derived resources containing gold, titanium and aluminum

a、b、c、d:步驟 a, b, c, d: steps

圖1:本發明含金、鈦、鋁濺鍍衍生資源物回收方法之步驟流程圖。 Figure 1: Step flow chart of the recovery method of sputtering derived resources containing gold, titanium, and aluminum according to the present invention.

圖2:本發明方法之具體的、較佳操作條件的流程示意圖。 Figure 2: A schematic flow diagram of specific and preferred operating conditions of the method of the present invention.

本發明涉及一種含金、鈦、鋁濺鍍衍生資源物回收方法A,如圖1及圖2所示,係提供具有PVD表面濺鍍鍍膜製程中的濺鍍腔室內所產生片狀的廢棄資源物之回收,通常每片衍生資源物的有價金屬比例大約是金30%、鈦10%、鋁60%,使用本發明回收技術可以達到零廢棄的完全回收,而本發明的回收方法係包含有:一破碎處理步驟a、一回收鋁步驟b、一回收金步驟c、一回收鈦步驟d。 The present invention relates to a recovery method A for sputtering-derived resources containing gold, titanium, and aluminum. As shown in Figures 1 and 2, it provides sheet-shaped waste resources generated in the sputtering chamber in the process of sputtering PVD surface coating. For the recycling of materials, usually the proportion of valuable metals in each piece of derived resource materials is about 30% of gold, 10% of titanium, and 60% of aluminum. The use of the recycling technology of the present invention can achieve complete recycling with zero waste, and the recycling method of the present invention includes : A crushing treatment step a, a recycling aluminum step b, a gold recycling step c, and a titanium recycling step d.

所述破碎處理步驟a,係針對濺鍍衍生資源物,以破碎方式俾利其與各金屬浸漬液有更大之接觸面積。 The crushing treatment step a is for the sputtering-derived resource material to use a crushing method to facilitate a larger contact area with each metal immersion liquid.

所述回收鋁步驟b,係將以一資源物放入20~30℃的5N~6N氫氧化鈉(NaOH)浸漬劑中,同時將其浸漬固液比條件設為3g/100ml,並浸漬15~25分鐘後,過濾後而得一含鋁浸漬液及一含金、鈦濾渣,再將該含鋁浸漬液經過pH調整沉澱後,即得氫氧化鋁Al(OH)3回收物,其pH調整沉澱方式係以鹽酸(HCl)溶液調節該含鋁浸漬液的酸鹼值至pH7。如圖2所示,其中該步驟的較佳操作條件設為使用25℃的6N氫氧化鈉浸漬劑,且浸漬20分鐘;特別一提,該回收鋁步驟b中所述浸漬劑濃度、浸漬固液比及浸漬時間等條件,均可以有多種搭配方式,並非為絕對。 In the step b of recovering aluminum, a resource is put into a 5N~6N sodium hydroxide (NaOH) impregnant at 20~30℃, while the impregnation solid-liquid ratio is set to 3g/100ml, and 15 ~25 minutes later, filtered to obtain an aluminum-containing impregnation solution and a gold and titanium-containing filter residue, and then after pH adjustment and precipitation of the aluminum-containing impregnation solution, the recovered aluminum hydroxide Al(OH) 3 is obtained. The adjustment of the precipitation method is to adjust the acid-base value of the aluminum-containing immersion solution to pH 7 with hydrochloric acid (HCl) solution. As shown in Figure 2, the optimal operating conditions for this step are set to use a 6N sodium hydroxide impregnant at 25°C and impregnate for 20 minutes; in particular, the concentration of the impregnant and the impregnating solid in step b of recovering aluminum Conditions such as liquid ratio and immersion time can be matched in many ways, which are not absolute.

所述回收金步驟c,係將前述含金、鈦濾渣放入60~80℃的5N~6N硝酸(HNO3)浸漬劑中,同時將其浸漬固液比條件設為1g/100ml,並浸漬

Figure 108115293-A0305-02-0005-1
Figure 108115293-A0305-02-0005-2
小時後,過濾而得高純度金回收物及一含鈦浸漬液。如圖2所示,其中該步驟的較佳操作條件設為使用70℃的6N硝酸浸漬劑,且浸漬4小時;特別一提,該回收金步驟c中所述浸漬劑濃度、浸漬固液比及浸漬時間等條件,均可以有多種搭配方式,並非為絕對。 The gold recovery step c is to put the aforementioned gold and titanium filter residue into a 5N-6N nitric acid (HNO 3 ) impregnant at 60-80°C, and at the same time set the impregnation solid-liquid ratio condition to 1g/100ml, and impregnate
Figure 108115293-A0305-02-0005-1
Figure 108115293-A0305-02-0005-2
After hours, filtered to obtain high-purity gold recovery and a titanium-containing impregnation solution. As shown in Figure 2, the optimal operating conditions for this step are set to use a 6N nitric acid impregnant at 70°C and impregnate for 4 hours; in particular, the impregnant concentration and impregnation solid-liquid ratio in the gold recovery step c Conditions such as immersion time, etc., can be matched in many ways, not absolute.

所述回收鈦步驟d,係將該含鈦浸漬液經過pH調整沉澱後,即得氫氧化鈦回收物,其pH調整沉澱方式,係以氫氧化鈉(NaOH)溶液調節該含鈦浸漬液的酸鹼值至pH7。 In the step d of recovering titanium, the titanium-containing impregnating solution undergoes pH adjustment and precipitation to obtain the recovered titanium hydroxide. The pH adjustment precipitation method is to adjust the titanium-containing impregnating solution with sodium hydroxide (NaOH) solution. The pH is up to pH7.

藉由上述各步驟流程構成本發明涉含金、鈦、鋁濺鍍衍生資源物回收方法,先以破碎方式以利其與金屬浸漬液有更大之接觸面積,之後再以5N~6N氫氧化鈉浸漬劑,固液比3g/100ml(浸漬樣品3g浸漬體積100ml)、20~30℃下予以浸漬15~25分鐘,可將含金、鈦、鋁金屬濺鍍衍生資源物中100%之鋁金屬予以浸漬溶蝕至最佳鋁浸漬液中。而之後再收集此最佳鋁浸漬液,以鹽酸調 整pH至7,在此pH條件下可達成100%之鋁沉澱回收,經過濾後可得「氫氧化鋁」產品,以供產業界使用。 The process of the above steps constitutes the recovery method of the sputtering-derived resources containing gold, titanium, and aluminum in the present invention. Firstly, it is crushed to facilitate a larger contact area with the metal immersion liquid, and then 5N~6N is used for hydrogenation. Sodium impregnant, solid-to-liquid ratio 3g/100ml (immersion sample 3g immersion volume 100ml), immersed at 20~30℃ for 15~25 minutes, can sputter 100% aluminum in derived resources of metals containing gold, titanium and aluminum The metal is immersed and corroded into the best aluminum immersion solution. And then collect the best aluminum dipping solution, adjust with hydrochloric acid Adjust the pH to 7, under this pH condition, 100% aluminum precipitation recovery can be achieved. After filtration, "aluminum hydroxide" products can be obtained for industrial use.

而經鋁浸漬溶蝕後再經過濾所得之含金、鈦濾渣則繼續進行鈦之浸漬溶蝕,以5N~6N硝酸浸漬劑,固液比0.5g/50ml(浸漬樣品0.5g浸漬體積50ml)、60~80℃下予以浸漬3~5小時,可將含金、鈦濾渣中100%之鈦金屬予以浸漬溶蝕之最佳鈦浸漬液中。之後,並收集此最佳鈦浸漬液,以氫氧化鈉調整pH至7,在此pH條件下可達成之鈦回收,經過濾後可得「氫氧化鈦」產品,以供產業界使用。而藉由鈦金屬浸漬溶蝕,將含金、鈦濾渣產品之鈦金屬100%去除,最後即可獲得高純度之「金」產品。 The gold and titanium filter residue obtained by aluminum immersion and dissolution and then filtration will continue to be impregnated and dissolved by titanium, with 5N~6N nitric acid impregnant, solid-to-liquid ratio 0.5g/50ml (immersion sample 0.5g immersion volume 50ml), 60 It is immersed for 3~5 hours at ~80℃, and 100% of the titanium metal in the filter residue containing gold and titanium can be immersed in the best titanium immersion solution for corrosion. After that, collect the best titanium impregnation solution, adjust the pH to 7 with sodium hydroxide, and recover the titanium that can be achieved under this pH condition. After filtration, the "titanium hydroxide" product can be obtained for industrial use. By impregnating and dissolving titanium metal, 100% of the titanium metal in the product containing gold and titanium filter residue is removed, and finally a high-purity "gold" product can be obtained.

本發明係關於一種「含金、鈦、鋁濺鍍衍生資源物回收方法」,且其各實施例的構成結構、製程均未曾見於諸書刊或公開使用,誠符合專利申請要件,懇請 鈞局明鑑,早日准予專利,至為感禱; 需陳明者,以上所述乃是本案之具體實施例及所運用之技術原理,若依本案之構想所作之改變,其所產生之功能作用仍未超出說明書及圖式所涵蓋之精神時,均應在本案之範圍內,合予陳明。 The present invention relates to a "recycling method for sputtering derived resources containing gold, titanium, and aluminum", and the structure and manufacturing process of each of its embodiments have not been seen in books or publicly used, and sincerely meets the requirements of a patent application. , Granting the patent as soon as possible, I am very grateful; For those who need to be clarified, the above are the specific embodiments of this case and the technical principles used. If the changes made according to the concept of this case, the resulting functional effects still do not exceed the spirit covered by the specification and drawings, All should be combined with Chen Ming within the scope of this case.

A:含金、鈦、鋁濺鍍衍生資源物回收方法 A: Recovery method of sputtering derived resources containing gold, titanium and aluminum

a、b、c、d:步驟 a, b, c, d: steps

Claims (1)

一種含金鈦鋁濺鍍衍生資源物回收方法,係包含有:一回收鋁步驟,係將以一資源物先經過破碎處理後,放入20~30℃、濃度為5N~6N、浸漬固液比條件設為3g/100ml的氫氧化鈉浸漬劑中,並浸漬15~25分鐘後,過濾後而得一含鋁浸漬液及一含金、鈦濾渣,再將該含鋁浸漬液經過pH調整沉澱後,即得氫氧化鋁回收物;前述pH調整沉澱方式,係以鹽酸溶液調節該含鋁浸漬液的酸鹼值至pH7;一回收金步驟,係將前述含金、鈦濾渣放入60~80℃、濃度為5N~6N、浸漬固液比條件設為1g/100ml的硝酸浸漬劑中,並浸漬3~5小時後,過濾而得高純度金回收物及一含鈦浸漬液;及一回收鈦步驟,係將該含鈦浸漬液經過pH調整沉澱後,其中該pH調整沉澱方式,係以氫氧化鈉溶液調節該含鈦浸漬液的酸鹼值至pH7,即得氫氧化鈦回收物。 A method for recovering resources derived from gold-titanium-aluminum sputtering includes: a step of recovering aluminum, in which a resource is first subjected to a crushing treatment, then placed in 20~30℃, concentration 5N~6N, impregnated solid liquid The ratio condition is set to 3g/100ml sodium hydroxide impregnant, and after immersing for 15-25 minutes, filtering to obtain an aluminum-containing impregnating solution and a gold and titanium-containing filter residue, and then the aluminum-containing impregnating solution is adjusted by pH After precipitation, the recovered aluminum hydroxide is obtained; the aforementioned pH adjustment precipitation method is to adjust the acid-base value of the aluminum-containing impregnation solution to pH 7 with a hydrochloric acid solution; a gold recovery step is to put the aforementioned gold and titanium filter residue into 60 ~80℃, concentration of 5N~6N, immersion in a nitric acid impregnant with a solid-to-liquid ratio of 1g/100ml, and immerse for 3~5 hours, then filter to obtain high-purity gold recovery and a titanium-containing impregnating solution; and The step of recovering titanium involves pH adjustment and precipitation of the titanium-containing impregnation solution, wherein the pH adjustment precipitation method is to adjust the acid-base value of the titanium-containing impregnation solution to pH 7 with sodium hydroxide solution to obtain titanium hydroxide recovery Things.
TW108115293A 2019-05-02 2019-05-02 Method for recovering gold-containing titanium-aluminum sputtering derived resources TWI697565B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271377A (en) * 2014-06-28 2016-01-27 郭耀 Titanium-containing concentrate recovery method
CN109546252A (en) * 2017-09-22 2019-03-29 银隆新能源股份有限公司 The recycling method of valuable metal in the cathode pole piece of waste and old lithium titanate battery

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271377A (en) * 2014-06-28 2016-01-27 郭耀 Titanium-containing concentrate recovery method
CN109546252A (en) * 2017-09-22 2019-03-29 银隆新能源股份有限公司 The recycling method of valuable metal in the cathode pole piece of waste and old lithium titanate battery

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